Hydrochloric Acid → HCID 178418412、化合物

HRID 1650

反応式

HRID 1650 の反応式
[C:1]([O:4][CH:5]1[CH2:10][CH2:9][CH:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH2:7][CH2:6]1)(=[O:3])[CH3:2].C=O.Cl.[CH2:20](Cl)[Cl:21]>[Cl-].[Zn+2].[Cl-]>[C:1]([O:4][C@H:5]1[CH2:10][CH2:9][C@H:8]([C:11]2[CH:16]=[CH:15][C:14]([CH2:20][Cl:21])=[CH:13][CH:12]=2)[CH2:7][CH2:6]1)(=[O:3])[CH3:2]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 6344DichloromethaneHCID 226557(4-Phenylcyclohexyl) acetate

生成物 1

HCID 178418412HCID 178418412、化合物

試薬・触媒・溶媒 1

HCID 3007855Zincchloride触媒

実験手順

A solution of 24.3 g (0.11 mol) of O-acetyl-4-phenylcyclohexanol in 1300 ml of methylene chloride is combined with 26.0 g (0.86 mol) of paraformaldehyde and 26.0 g (0.19 mol) of zinc chloride. Hydrogen chloride is introduced into this suspension, with stirring, for 2.5 hours, whilst the temperature rises to about 30° C. and a substantially homogeneous solution is formed. The mixture is then allowed to react for 15 hours at ambient temperature and the reaction mixture is then hydrolysed with stirring in about 1.5 litres of ice water. The organic phase is separated off, the aqueous phase is extracted with methylene chloride again and the two organic phases are combined. They are washed until neutral, dried and evaporated in vacuo. The yellow oil remaining is crystallised by trituration with diisopropylether and the solid product is recrystallised from diisopropylether. White crystals are obtained, melting point 87°-89° C.

後処理

  1. customrises to about 30° C.
  2. customa substantially homogeneous solution is formed
  3. customto react for 15 hours at ambient temperature
  4. customThe organic phase is separated off
  5. extractionthe aqueous phase is extracted with methylene chloride again
  6. washThey are washed until neutral,
  7. customdried
  8. customevaporated in vacuo
  9. customThe yellow oil remaining is crystallised by trituration with diisopropylether
  10. customthe solid product is recrystallised from diisopropylether
  11. customWhite crystals are obtained

出典と根拠

ORDレコード
ord-989f1c45e316471198b7f2d873102bdb
出典データセット
uspto-grants-1998_03
特許番号
US05726205

関連ノート

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